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1.
Hans-Rudolf Buser Michael Oehme Walter Vetter Bernd Luckas 《Fresenius' Journal of Analytical Chemistry》1993,347(12):502-512
Summary Conventional electron ionization (EI) mass spectrometry (MS) and MS/MS techniques were applied to the analysis of two abundant octa and nonachlorobornanes isolated from seals of the Baltic sea and originating from technical toxaphene. The exact sterical structures of the two compounds were previously determined using nuclear magnetic resonance (NMR) spectroscopy by two independent research groups. The MS and MS/MS data generated in this study allowed partial structure elucidation of these polychlorobornanes, in particular revealing the distribution of the Cl substituents between the six-membered carbon ring, the bridge and the bridgehead in the parent bornane structure. Fragmentation of the six-membered carbon ring and the bridge by retro-Diels-Alder (RDA) and related mechanisms was discovered by studying specific parent/daughter ion transitions. The detailed fragmentation pathways formulated may be applicable to the structure elucidation of other toxaphene congeners and the monitoring of strategic transitions is highly selective for the detection of these compounds in technical toxaphene and in environmental samples. 相似文献
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Walter Selig 《Fresenius' Journal of Analytical Chemistry》1969,247(5-6):294-296
Summary A new complexometric method for the determination of phosphorus in organic compounds is described. After combustion in an oxygen-flask, phosphorus is precipitated as cerous phosphate. The excess cerous ion is back-titrated at pH 6–7 with EDTA in the presence of methylthymol blue or xylenol orange indicators. Alkaline hypobromite is used as an absorbent. Tight clamping of the paper carrier in the platinum holder insures complete combustion.
This work was performed under the auspices of the U.S. Atomic Energy Commission. 相似文献
Komplexometrische Titration von Phosphor in organischen Verbindungen
Zusammenfassung Die Probe wird im Sauerstoffkolben nach Schöniger verbrannt und der Phosphor als Cer(III)-phosphat ausgefällt. Der Überschuß an Cer(III) wird bei pH 6–7 mit ÄDTA zurücktitriert, wobei Methylthymolblau oder Xylenolorange als Indicator dient. Als Absorptionsmittel wird alkalische Hypobromitlösung verwendet. Um eine vollständige Verbrennung zu gewährleisten, ist es wichtig, daß das Papier mit der Probe fest am Platinhalter angeklammert wird.
This work was performed under the auspices of the U.S. Atomic Energy Commission. 相似文献
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Li2SnO3 crystallises monoclinic, C, with a = 5.295, b = 9.184, c = 10.032 Å and β = 100.13°; Z = 8. The positions of Sn were obtained from PATTERSON maps and the positions of O and Li by FOURIER difference method. Parameters were refined by least squares-method [1462 reflexes (h 01)–(h 71); R = 10.5%]. The average distances of Li? O are 2.07 Å, and 2.20 Å for Sn? O. The Li2SnO3 structure can be derived from the NaCl type: in a cubic closest packing of oxygen 2/3 of the octahedral holes are occupied by lithium and 1/3 by tin. 相似文献
7.
Gerald Koitz Walter Fabian Hans-Werner Schmidt Hans Junek 《Monatshefte für Chemie / Chemical Monthly》1981,112(8-9):973-985
The synthesis of several 2-aminopyridines is described. The reaction of tetracyanoethylene with 3-imino-propane-carbonitrile gives 2-amino-3,4,5-tricyano-pyridines with alkyl and aryl-substituents, resp., in position 6. Nucleophilic substitution of 2-amino-6-chloro-3,5-dicyanopyridines and 2-amino-6-chloro-3,4,5-tricyano-pyridines with phenolates leads to a variety of pyridines. Spectroscopical data of absorption and fluorescence are presented and the influence of the cyano groups is discussed. The results are in good agreement with quantum chemical calculations (PPP).
Herrn Univ-Prof. Dr.A. Holasek zum 60. Geburtstag gewidmet. 相似文献
8.
Magnetochemistry of Divalent Silver. New Fluoroargentates(II): Cs2AgF4, Rb2AgF4, and K2AgF4 Hitherto unknown blue compounds Rb2AgF4 and Cs2AgF4 are prepared. Guinier patterns show, that Cs2AgF4 cristallise in the K2NiF4 structure (a = 4.581, c = 14.192 Å). The structure of the Rb-compound is still unknown. The magnetic behaviour of K2AgF4, Rb2AgF4, and Cs2AgF4 is discussed. 相似文献
9.
About Perrhenates. 1. On LiReO4 For the very first time anhydrous LiReO4 was prepared in transparent, colourless single crystals from Li2O2 and Re2O7 (closed Au-pipe; 350°C; 14 d). The crystal structure, P1 , with a = 9.652(1), b = 8.455(1), c = 6.928(1) Å, α = 101,53° (1), β = 106.55° (1), γ = 97.22° (1), Z = 6, dx = 4.92 g/cm3, dpyk = 4,81 g/cm3 was solved (four-circle-diffractometer data PW 1100, 2151 I0 (hkl), AgKα; R = 0.073, Rw = 0.076). There are three kinds of functionally different Li+. The Madelung Part of the Lattice Energy, MAPLE, was calculated. 相似文献
10.
The purpose of this communication is to describe the preparation and some properties of the first two synthetic peptides containing D - and L -γ-carboxyglutamic acid. Use was made of N-protected γ,γ′-di-t-butyl-γ-carboxyglutamic acids (D , L , and DL ) described earlier [1 a]. Preliminary 1H-NMR. data (360 MHz) indicate a restricted rotation of the Gla side chain in the free amino acid as well as in the C-terminal Gla of Gla-Gla in H2O solution at acid pH. The proton dissociation from Gla and Gla-Gla was studied by potentiometric titration and NMR. methods. The pH titration in the presence of Ca2+ ions shows that Gla-Gla has a much higher association constant for this cation than Gla. It is almost as great as that of prothrombin (pCa2+ = 3.2 vs. 3.5). 相似文献